FACILE REDUCTION OF AROMATIC NITRO COMPOUNDS WITH HYDROIODIC ACID UNDER MICROWAVE IRRADIATION ON SOLID SUPPORT

Reduction of aromatic nitro compounds to amine with hydroiodic acid was revisited. Under microwave irradiation on solid support the reduction proceeded efficiently and rapidly.     

SELECTIVE OXIDATION OF BENZYLIC ALCOHOLS USING CAN SUPPORTED ONTO SILICA GEL UNDER MICROWAVE IRRADIATION

Cerium ammonium nitrate (CAN) adsorbed on HNO ₃ /silica gel is a mild reagent for selective oxidation of benzylic alcohols to the corresponding aldehydes under microwave irradiation in solventless system.     

Preparation and Characterization of Cu2S Nanoparticles Via Ultrasonic Method

This study reports on the synthesis of Cu₂S nanoparticles via an ultrasonic method by employing Na₂SO₃ as a reducing agent. Morphology, structure, and composition of the obtained products were characterized by X-ray diffraction, energy dispersive X-ray analysis, scanning electron microscope and photoluminescence spectroscopy. The effects of time and power of irradiation were studied.     

A quantitative and comprehensive method to analyze human milk oligosaccharide structures in the urine and feces of infants

Human milk oligosaccharides (HMOs), though non-nutritive to the infant, shape the intestinal microbiota and protect against pathogens during early growth and development. Infant formulas with added galacto-oligosaccharides have been developed to mimic the beneficial effects of HMOs. Premature infants have an immature immune system and a leaky gut and are thus highly susceptible to opportunistic infections. A method employing nanoflow liquid chromatography time-of-flight mass spectrometry (MS) is presented to simultaneously identify and quantify HMOs in the feces and urine of infants, of which 75 HMOs have previously been fully structurally elucidated. Matrix-assisted laser desorption/ionization Fourier transform ion cyclotron resonance MS was employed for high-resolution and rapid compositional profiling. To demonstrate this novel method, samples from mother–infant dyads as well as samples from infants receiving infant formula fortified with dietary galacto-oligosaccharides or probiotic bifidobacteria were analyzed. Ingested oligosaccharides are demonstrated in high abundance in the infant feces and urine. While the method was developed to examine specimens from preterm infants, it is of general utility and can be used to monitor oligosaccharide consumption and utilization in term infants, children, and adults. This method may therefore provide diagnostic and therapeutic opportunities.

Recent advances in synthesis of 2-pyridones: a key heterocycle is revisited

Owing to the versatile applications in different areas including biology, natural compounds, dyes, and fluorescent materials, the synthesis of 2-pyridone compounds is an important research field and has attracted a great deal of attention. In this review, 2-pyridones new synthetic methods are classified to tree classes including reactions based on pyridine rings, cyclization, and cycloaddition reactions.     

Fabrication and application of a new modified electrochemical sensor using nano-silica and a newly synthesized Schiff base for simultaneous determination of Cd,Cu and Hg ions in water and some foodstuff samples

A new chemically modified carbon paste electrode was constructed and used for rapid, simple, accurate, selective and highly sensitive simultaneous determination of cadmium, copper and mercury using square wave anodic stripping voltammetry (SWASV). The carbon paste electrode was modified by N,N′-bis(3-(2-thenylidenimino)propyl)piperazine coated silica nanoparticles. Compared with carbon paste electrode, the stripping peak currents had a significant increase at the modified electrode. Under the optimized conditions (deposition potential, −1.100 V vs. Ag/AgCl; deposition time, 60 s; resting time, 10 s; SW frequency, 25 Hz; pulse amplitude, 0.15 V; dc voltage step height, 4.4 mV), the detection limit was 0.3, 0.1 and 0.05 ng mL⁻¹ for the determination of Cd²⁺, Cu²⁺ and Hg²⁺, respectively. The complexation reaction of the ligand with several metal cations in methanol was studied and the stability constants of the complexes were obtained. The effects of different cations and anions on the simultaneous determination of metal ions were studied and it was found that the electrode is highly selective for the simultaneous determination of Cd²⁺, Cu²⁺ and Hg²⁺. Furthermore, the present method was applied to the determination of Cd²⁺, Cu²⁺ and Hg²⁺ in water and some foodstuff samples.     

Adsorptive Stripping Differential Pulse Voltammetric Determination of Risperidone with a Multi‐Walled Carbon Nanotube‐Ionic Liquid Paste Modified Glassy Carbon Electrode

A new composite electrode has been fabricated based on coating multi‐walled carbon nanotubes (MWCNTs) and n‐octylpyridinum hexafluorophosphate (OPPF₆) ionic liquid composite on a glassy carbon (GC) electrode (OPPF₆‐MWCNTs/GCE). This electrode shows very attractive electrochemical performances for electrooxidation of risperidone (RIS) compared to conventional electrodes using carbon and mineral oil, notably improved sensitivity and stability. The oxidation peak potentials in cyclic voltammogram of RIS on the OPPF₆‐MWCNTs/GCE was occurred around 230 mV vs. SCE at Britton–Robinson (B–R) buffer (pH 4.0) at scan rate of 100 mV s^?1. The electrochemical parameters such as diffusion coefficient (D), charge transfer coefficient (α) and the electron transfer rate constant (k/_s) were determined using cyclic voltammetry. Under the optimized conditions, the peak current was linear to risperidone concentration over the concentration range of 10–200 nM with sensitivity of 0.016 μA/nM^?1 using differential pulse voltammetry. The detection limit was 6.54 nM (S/N = 3). The electrode also displayed good selectivity and repeatability. In the presence of clozapine (CLZ) the response of RIS kept almost unchanged. Thus this electrode could find application in the determination of RIS in some real samples. The analytical performance of the OPPF₆‐MWCNTs/GCE was demonstrated for the determination of RIS in human serum and pharmaceutical samples.     

Homogeneous Liquid–Liquid Microextraction Via Flotation Assistance (HLLME-FA) Method for the Pretreatment of Organochlorine Pesticides in Aqueous Samples and Determination by GC–MS

This work proposes a new, rapid and simple homogeneous liquid–liquid microextraction via flotation assistance technique for the analysis of six organochlorine pesticides in water samples. A special extraction cell was used to facilitate collection of the low-density solvent extract. No centrifugation was required in this procedure. Determination was carried using gas chromatography–mass spectrometry. The water sample solution was then added into the extraction cell containing appropriate mixture of extract and homogeneous solvents. In the first step, a homogeneous solution and then with the continuation of water sample injection, a cloudy solution was formed. Using air flotation, the organic solution was collected at the conical part of the designed cell. The optimized levels of effective parameters were found based on response surface methodology approach. Applying the optimized conditions to the system understudy, the limits of detection of all target analytes were obtained in the range of 1.4–7 ng mL^?1, while the precisions were found to be in the range of 11.08–14.87 (RSD, n = 3). The linearity of the method lay in the range of 10–150 ng mL^?1 with the coefficients of correlation (r ² ) ranging from 0.998 to 0.999.     

Synthesis of a New Heteropolytopic Cryptand Through Schiff Base Condensation in the Presence of Ba(II) Ion

A new Schiff base cryptand (L) has been prepared via [2 + 2] condensation of 1,3,5-tris(2-formylphenoxymethyl)benzene (1) with 1,3,5-tris(aminomethyl)benzene trishydrochloride (2) in the presence of Ba(II) ion. The analytical data show that the Ba(II) cation is not retained by the product. Thus it seems that the role of the Ba(II) ion is to organize the transition state preceding the formation of the cryptand.     

Oxidation of 1,4-Dihydropyridines under Mild and Heterogeneous Conditions

A combination of NaHSO₄.H₂O and NaNO₂ in the presence of wet SiO₂ was used as an effective oxidizing agent for the oxidation of dihydropyridines to their corresponding pyridine derivatives at room temperature with excellent yields.